反应 #1880947

ord-d5fe10d189b6424ebdad4e166a453247

反应方程式

CCN(CC)CC
triethylamine
N#Cc1ccc(N=Nc2ccc(OCCO)c(C#N)c2)cc1
4-(2-hydroxyethyloxy)-3,4′-dicyanoazobenzene
C=C(C)C(=O)Cl
methacrylic acid chloride
C=C(C)C(=O)OCCOc1ccc(N=Nc2ccc(C#N)cc2)cc1C#N
4-(2-Methacryloyloxyethyloxy)-3,4′-dicyanoazobenzene

反应条件

温度
65°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤The precipitate is filtered off with suction
  2. 2
    其他dried
  3. 3
    其他Purification

实验过程

5.8 g (4-(2-hydroxyethyloxy)-3,4′-dicyanoazobenzene are dissolved in 15 ml dioxane at 65° C.; 2.4 g triethylamine are added. A solution of 3.1 g methacrylic acid chloride in 3 ml dioxane is added and the reaction mixture is stirred at 65° C. for 2 h and then introduced into 350 ml ice-water. The precipitate is filtered off with suction and dried. Purification is carried out by chromatography on silica gel in toluene/THF (½). The yield of 4-(2-methacryloyloxyethyloxy)-3,4′-dicyanoazobenzene is 5.9 g. M.p.=110° C.; max=352 nm (DMF).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07022460B2uspto-grants-2006_04